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目的:建立双柏散中槲皮苷和薄荷脑的含量测定方法,为双柏制剂的质量控制与化学物质基础研究提供分析手段。方法:采用HPLC法测定槲皮苷含量。采用Eclipse XDB C18为色谱柱;流动相为乙腈-0.01mol.L-1磷酸二氢钾溶液-冰醋酸(16∶84∶2.1);检测波长为352 nm;流速为1 mL.min-1;柱温为40℃。以水杨酸甲酯为内标物,采用GC法测定薄荷脑的含量。以HP-5为色谱柱,进样口温度为210℃;FID检测器,检测器温度为280℃,程序升温:初始温度50℃,保持2 min后,以60℃.min-1升至120℃后保持5 min,再以10℃.min-1升至150℃后,再以60℃.min-1升至235℃后保持10 min;流速为1.1 mL.min-1,分流比为1∶1。结果:槲皮苷在0.020 48~1.228 8μg范围内线性关系良好(r=0.999 9),平均加样回收率为97.20%(RSD=1.75%);薄荷脑在0.002 73~0.087 36μg范围内线性关系良好(r=0.999 5),平均加样回收率为99.97%(RSD=2.88%)。双柏散中槲皮苷、薄荷脑含量分别为0.851 9~1.286 3 mg.g-1、0.068 3~0.855 6 mg.g-1。结论方法简便、重复性好,为双柏制剂的质量控制与化学物质基础研究提供了一定的分析手段。
OBJECTIVE: To establish a method for the determination of quercitrin and menthol in Shuangbai San, and provide analysis methods for the quality control and basic research of chemical substances of Shuangbai. Methods: The quercitrin content was determined by HPLC. Eclipse XDB C18 was used as the column; the mobile phase was acetonitrile-0.01mol.L-1 potassium dihydrogen phosphate solution-glacial acetic acid (16:84:2.1); the detection wavelength was 352 nm; the flow rate was 1 mL.min-1; The column temperature is 40°C. Methyl salicylate was used as the internal standard and the content of menthol was determined by GC. HP-5 column, inlet temperature 210 °C; FID detector, detector temperature is 280 °C, program temperature: initial temperature of 50 °C, after 2 min, to 60 °C.min-1 rose to 120 Keep at 5 °C for 5 min, then increase at 10 °C.min-1 to 150 °C, then increase at 60 °C.min-1 to 235 °C and hold for 10 min; flow rate is 1.1 mL.min-1, split ratio is 1 1:1. RESULTS: The linearity of quercitrin was good in the range of 0.020 48~1.228 8 μg (r=0.999 9), the average recovery was 97.20% (RSD=1.75%), and the linear relationship of menthol in the range of 0.002 73 to 0.087 36 μg. Good (r=0.999 5), the average recovery was 99.97% (RSD=2.88%). The contents of quercitrin and menthol in Shuangbai San were 0.851 9-1.286 3 mg.g-1 and 0.068 3-8.855 6 mg.g-1, respectively. Conclusions The method is simple and reproducible. It provides a certain analysis method for quality control and basic research of chemical substances of Shuangbai preparations.